+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0059p21 started at 08:44:04 on 07-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0059p21 in P2(1) CELL 0.71073 8.2165 7.0534 10.0677 90.000 104.266 90.000 ZERR 2.00 0.0004 0.0005 0.0007 0.000 0.004 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 14 36 4 12 V = 565.47 F(000) = 244.0 Mu = 0.12 mm-1 Cell Wt = 452.47 Rho = 1.329 MERG 4 OMIT -3.00 55.00 OMIT 0 0 1 OMIT -2 0 3 OMIT -6 -2 5 OMIT 1 0 0 OMIT -4 -2 2 EXTI 0.05774 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W O2W H21W O2W H22W DANG 1.35 0.02 H1W H2W H21W H22W HTAB N24 O1A HTAB N24 O2A HTAB O1W O2B HTAB O2W O2A EQIV_$1 x+1, y, z HTAB N21 O2B_$1 HTAB N21 O1B_$1 EQIV_$2 -x+1, y-1/2, -z+2 HTAB N24 O1A_$2 EQIV_$3 -x, y-1/2, -z+1 HTAB O1W O2B_$3 HTAB O2W O1W_$3 FMAP 2 PLAN 10 SIZE 0.03 0.11 0.20 ACTA 50 BOND $H WGHT 0.04950 L.S. 4 TEMP -153.00 FVAR 1.86793 MOLE 1 C1 1 0.190262 0.203323 0.875254 11.00000 0.02016 0.02753 = 0.02391 0.00220 0.00684 -0.00026 C2 1 0.148772 0.051413 0.760222 11.00000 0.02130 0.02603 = 0.02932 0.00408 0.00782 0.00108 O1A 4 0.343256 0.214667 0.940616 11.00000 0.01807 0.03229 = 0.03063 -0.00693 0.00320 0.00033 O1B 4 0.073848 0.298382 0.897099 11.00000 0.01851 0.04442 = 0.04503 -0.01648 0.00509 0.00180 O2A 4 0.260621 -0.061924 0.751217 11.00000 0.02366 0.03426 = 0.04144 -0.00836 0.00260 0.00668 O2B 4 0.001664 0.060469 0.682270 11.00000 0.02030 0.03554 = 0.03536 -0.00593 0.00243 -0.00017 MOLE 2 C22 1 0.624232 0.131283 0.667013 11.00000 0.02091 0.03366 = 0.02737 -0.00284 0.00416 -0.00089 AFIX 23 H22A 2 0.647771 0.093205 0.578950 11.00000 -1.20000 H22B 2 0.507608 0.179534 0.647785 11.00000 -1.20000 AFIX 0 C23 1 0.642316 -0.038240 0.761030 11.00000 0.02302 0.02860 = 0.03758 -0.00469 0.00977 -0.00156 AFIX 23 H23A 2 0.561246 -0.137682 0.718189 11.00000 -1.20000 H23B 2 0.756988 -0.091175 0.775869 11.00000 -1.20000 AFIX 0 C25 1 0.723249 0.175272 0.959134 11.00000 0.02282 0.03248 = 0.02857 -0.00196 0.00595 -0.00001 AFIX 23 H25A 2 0.841062 0.130448 0.982648 11.00000 -1.20000 H25B 2 0.694492 0.214239 1.045040 11.00000 -1.20000 AFIX 0 C26 1 0.706814 0.341827 0.864862 11.00000 0.01952 0.02755 = 0.03006 -0.00401 0.00529 0.00394 AFIX 23 H26A 2 0.786420 0.442301 0.908259 11.00000 -1.20000 H26B 2 0.591592 0.393868 0.847572 11.00000 -1.20000 AFIX 0 C27 1 0.740116 0.449739 0.638977 11.00000 0.03375 0.03162 = 0.03878 0.01124 0.00953 0.00441 AFIX 137 H27A 2 0.630447 0.512339 0.622164 11.00000 -1.50000 H27B 2 0.759721 0.406275 0.551774 11.00000 -1.50000 H27C 2 0.828315 0.539539 0.682218 11.00000 -1.50000 AFIX 0 N21 3 0.742959 0.283543 0.731697 11.00000 0.02080 0.02338 = 0.03071 0.00469 0.00600 0.00498 AFIX 13 H21 2 0.850724 0.232800 0.751406 11.00000 0.03116 AFIX 0 N24 3 0.610846 0.018363 0.894581 11.00000 0.01909 0.02812 = 0.02938 0.00399 0.00707 0.00160 AFIX 23 H24A 2 0.500837 0.056154 0.881314 11.00000 -1.20000 H24B 2 0.627562 -0.084482 0.952569 11.00000 -1.20000 AFIX 0 MOLE 3 O1W 4 -0.150072 -0.187782 0.487956 11.00000 0.03885 0.03401 = 0.03545 -0.00574 0.00345 -0.00138 H1W 2 -0.089997 -0.256457 0.449921 11.00000 0.06440 H2W 2 -0.080210 -0.122880 0.546865 11.00000 0.11373 MOLE 4 O2W 4 0.355508 -0.417196 0.675174 11.00000 0.02759 0.03542 = 0.05350 -0.00383 0.01031 0.00110 H21W 2 0.299695 -0.320664 0.685031 11.00000 0.04845 H22W 2 0.282143 -0.505474 0.646845 11.00000 0.06378 HKLF 4 Covalent radii and connectivity table for 06skc0059p21 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2A O2B C1 O1A - C1 O1B - C1 O2A - C2 O2B - C2 C22 - N21 C23 C23 - N24 C22 C25 - N24 C26 C26 - C25 N21 C27 - N21 N21 - C22 C27 C26 N24 - C25 C23 O1W - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $2 -x+1, y-1/2, -z+2 $3 -x, y-1/2, -z+1 Floating origin restraints generated 7124 Reflections read, of which 33 rejected -9 =< h =< 9, -7 =< k =< 7, -11 =< l =< 11, Max. 2-theta = 46.70 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 2 3 120.70 36.82 2 201.17 -6 3 4 208.25 8.92 7 55.07 -6 2 5 208.32 22.12 2 118.13 3 Inconsistent equivalents 738 Unique reflections, of which 0 suppressed R(int) = 0.0657 R(sigma) = 0.0537 Friedel opposites merged Maximum memory for data reduction = 2042 / 7515 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 2470 / 193805 wR2 = 0.0788 before cycle 1 for 738 data and 155 / 155 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.014 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.064; Restrained GooF = 1.059 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86791 0.00900 -0.002 OSF 2 0.05773 0.01161 -0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.008 for U11 H21W Max. shift = 0.000 A for H21W Max. dU = 0.000 for H21W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2470 / 193805 wR2 = 0.0788 before cycle 2 for 738 data and 155 / 155 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.014 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.058 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86790 0.00900 -0.001 OSF 2 0.05772 0.01161 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.005 for U11 H21W Max. shift = 0.000 A for H21W Max. dU = 0.000 for H21W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2470 / 193805 wR2 = 0.0788 before cycle 3 for 738 data and 155 / 155 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.014 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.058 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86790 0.00900 0.000 OSF 2 0.05772 0.01161 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U11 H21W Max. shift = 0.000 A for H21W Max. dU = 0.000 for H21W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2470 / 193805 wR2 = 0.0788 before cycle 4 for 738 data and 155 / 155 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.014 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.059 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86790 0.00900 0.000 OSF 2 0.05772 0.01161 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 H21W Max. shift = 0.000 A for H21W Max. dU = 0.000 for H21W Largest correlation matrix elements -0.731 z H2W / y H2W 0.557 U13 C2 / U33 C2 0.514 U13 O2A / U33 O2A -0.649 y H22W / x H22W 0.534 U13 O1W / U33 O1W 0.513 U13 N24 / U33 N24 0.613 z H1W / x H1W 0.524 U13 O2B / U11 O2B 0.506 U13 N24 / U11 N24 0.596 EXTI / OSF 0.517 U13 O1B / U33 O1B 0.506 U13 C23 / U33 C23 0.594 y H22W / y H21W 0.515 U13 C27 / U33 C27 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H22A 0.6478 0.0932 0.5789 23 0.990 0.000 C22 N21 C23 H22B 0.5076 0.1795 0.6478 23 0.990 0.000 C22 N21 C23 H23A 0.5612 -0.1377 0.7182 23 0.990 0.000 C23 N24 C22 H23B 0.7570 -0.0912 0.7759 23 0.990 0.000 C23 N24 C22 H25A 0.8411 0.1304 0.9826 23 0.990 0.000 C25 N24 C26 H25B 0.6945 0.2142 1.0450 23 0.990 0.000 C25 N24 C26 H26A 0.7864 0.4423 0.9083 23 0.990 0.000 C26 C25 N21 H26B 0.5916 0.3939 0.8476 23 0.990 0.000 C26 C25 N21 H27A 0.6304 0.5123 0.6222 137 0.980 0.000 C27 N21 H27A H27B 0.7597 0.4063 0.5518 137 0.980 0.000 C27 N21 H27A H27C 0.8283 0.5395 0.6822 137 0.980 0.000 C27 N21 H27A H21 0.8507 0.2328 0.7514 13 0.930 0.000 N21 C22 C27 C26 H24A 0.5008 0.0562 0.8813 23 0.920 0.000 N24 C25 C23 H24B 0.6276 -0.0845 0.9526 23 0.920 0.000 N24 C25 C23 06skc0059p21 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.19026 0.20332 0.87525 1.00000 0.02016 0.02753 0.02391 0.00220 0.00684 -0.00026 0.02362 0.00711 0.00044 0.00054 0.00036 0.00000 0.00207 0.00202 0.00209 0.00180 0.00168 0.00187 0.00090 C2 0.14877 0.05141 0.76022 1.00000 0.02130 0.02603 0.02932 0.00409 0.00782 0.00108 0.02527 0.00760 0.00044 0.00054 0.00038 0.00000 0.00206 0.00216 0.00224 0.00179 0.00174 0.00186 0.00089 O1A 0.34326 0.21467 0.94062 1.00000 0.01807 0.03228 0.03063 -0.00693 0.00320 0.00032 0.02748 0.00454 0.00027 0.00034 0.00026 0.00000 0.00136 0.00155 0.00149 0.00127 0.00112 0.00117 0.00068 O1B 0.07385 0.29838 0.89710 1.00000 0.01851 0.04442 0.04503 -0.01648 0.00509 0.00180 0.03647 0.00532 0.00032 0.00048 0.00029 0.00000 0.00133 0.00166 0.00181 0.00161 0.00127 0.00133 0.00076 O2A 0.26062 -0.06192 0.75122 1.00000 0.02366 0.03426 0.04144 -0.00837 0.00260 0.00668 0.03407 0.00494 0.00030 0.00038 0.00028 0.00000 0.00152 0.00160 0.00174 0.00141 0.00133 0.00128 0.00074 O2B 0.00166 0.06047 0.68227 1.00000 0.02030 0.03554 0.03536 -0.00593 0.00243 -0.00017 0.03118 0.00508 0.00029 0.00042 0.00026 0.00000 0.00143 0.00156 0.00163 0.00135 0.00125 0.00130 0.00069 C22 0.62423 0.13128 0.66701 1.00000 0.02091 0.03366 0.02737 -0.00284 0.00416 -0.00089 0.02763 0.00771 0.00048 0.00055 0.00040 0.00000 0.00184 0.00231 0.00227 0.00178 0.00178 0.00162 0.00097 H22A 0.64777 0.09321 0.57895 1.00000 0.03315 0.00000 0.00000 H22B 0.50761 0.17953 0.64779 1.00000 0.03315 0.00000 0.00000 C23 0.64232 -0.03824 0.76103 1.00000 0.02302 0.02860 0.03758 -0.00469 0.00977 -0.00156 0.02933 0.00787 0.00050 0.00053 0.00042 0.00000 0.00197 0.00219 0.00223 0.00189 0.00182 0.00169 0.00093 H23A 0.56125 -0.13768 0.71819 1.00000 0.03520 0.00000 0.00000 H23B 0.75699 -0.09117 0.77587 1.00000 0.03520 0.00000 0.00000 C25 0.72325 0.17527 0.95913 1.00000 0.02282 0.03247 0.02857 -0.00196 0.00595 -0.00001 0.02802 0.00711 0.00043 0.00055 0.00038 0.00000 0.00184 0.00219 0.00217 0.00188 0.00164 0.00185 0.00089 H25A 0.84106 0.13045 0.98265 1.00000 0.03362 0.00000 0.00000 H25B 0.69449 0.21424 1.04504 1.00000 0.03362 0.00000 0.00000 C26 0.70681 0.34183 0.86486 1.00000 0.01952 0.02755 0.03006 -0.00401 0.00529 0.00394 0.02585 0.00778 0.00047 0.00052 0.00041 0.00000 0.00200 0.00215 0.00218 0.00171 0.00176 0.00163 0.00090 H26A 0.78642 0.44230 0.90826 1.00000 0.03102 0.00000 0.00000 H26B 0.59159 0.39387 0.84757 1.00000 0.03102 0.00000 0.00000 C27 0.74012 0.44974 0.63898 1.00000 0.03375 0.03162 0.03878 0.01123 0.00952 0.00441 0.03461 0.00855 0.00054 0.00054 0.00042 0.00000 0.00219 0.00221 0.00242 0.00199 0.00191 0.00193 0.00096 H27A 0.63045 0.51234 0.62217 1.00000 0.05192 0.00000 0.00000 H27B 0.75972 0.40628 0.55177 1.00000 0.05192 0.00000 0.00000 H27C 0.82832 0.53954 0.68222 1.00000 0.05192 0.00000 0.00000 N21 0.74296 0.28354 0.73170 1.00000 0.02080 0.02338 0.03071 0.00469 0.00600 0.00498 0.02502 0.00634 0.00037 0.00046 0.00030 0.00000 0.00156 0.00163 0.00182 0.00155 0.00136 0.00138 0.00076 H21 0.85072 0.23280 0.75141 1.00000 0.03117 0.00000 0.01092 N24 0.61085 0.01836 0.89458 1.00000 0.01909 0.02812 0.02938 0.00400 0.00707 0.00160 0.02534 0.00601 0.00038 0.00042 0.00031 0.00000 0.00158 0.00178 0.00186 0.00146 0.00141 0.00136 0.00078 H24A 0.50084 0.05615 0.88131 1.00000 0.03041 0.00000 0.00000 H24B 0.62756 -0.08448 0.95257 1.00000 0.03041 0.00000 0.00000 O1W -0.15007 -0.18778 0.48796 1.00000 0.03885 0.03401 0.03545 -0.00574 0.00345 -0.00137 0.03710 0.00584 0.00036 0.00044 0.00031 0.00000 0.00163 0.00173 0.00172 0.00154 0.00154 0.00154 0.00074 H1W -0.08999 -0.25646 0.44993 1.00000 0.06439 0.09569 0.00576 0.00595 0.00504 0.00000 0.01743 H2W -0.08023 -0.12288 0.54688 1.00000 0.11389 0.04183 0.00637 0.00893 0.00581 0.00000 0.02755 O2W 0.35551 -0.41720 0.67517 1.00000 0.02759 0.03541 0.05350 -0.00383 0.01031 0.00110 0.03878 0.00609 0.00035 0.00043 0.00032 0.00000 0.00150 0.00176 0.00199 0.00157 0.00140 0.00150 0.00078 H21W 0.29973 -0.32064 0.68502 1.00000 0.04823 0.07988 0.00513 0.00430 0.00498 0.00000 0.01409 H22W 0.28213 -0.50546 0.64684 1.00000 0.06383 0.05695 0.00515 0.00484 0.00522 0.00000 0.01662 Final Structure Factor Calculation for 06skc0059p21 in P2(1) Total number of l.s. parameters = 155 Maximum vector length = 511 Memory required = 2317 / 25046 wR2 = 0.0788 before cycle 5 for 738 data and 2 / 155 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.014 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.059 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0344 for 641 Fo > 4sig(Fo) and 0.0462 for all 738 data wR2 = 0.0788, GooF = S = 1.063, Restrained GooF = 1.059 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0286 0.0233 0.0190 C1 0.0321 0.0233 0.0204 C2 0.0395 0.0250 0.0179 O1A 0.0629 0.0282 0.0182 O1B 0.0522 0.0297 0.0203 O2A 0.0429 0.0308 0.0198 O2B 0.0348 0.0274 0.0206 C22 0.0396 0.0266 0.0218 C23 0.0334 0.0279 0.0228 C25 0.0346 0.0255 0.0174 C26 0.0471 0.0336 0.0232 C27 0.0330 0.0253 0.0168 N21 0.0328 0.0248 0.0185 N24 0.0458 0.0376 0.0279 O1W 0.0547 0.0349 0.0267 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.037 0.058 0.078 0.094 0.112 0.134 0.163 0.195 0.259 1.000 Number in group 76. 72. 76. 74. 75. 73. 73. 73. 72. 74. GooF 0.825 0.810 1.218 1.072 0.993 0.880 0.939 1.008 1.157 1.525 K 1.834 0.989 1.001 1.062 0.986 0.996 0.987 0.999 1.024 1.010 Resolution(A) 0.90 0.93 0.96 1.00 1.04 1.10 1.17 1.29 1.43 1.77 inf Number in group 76. 73. 73. 73. 77. 71. 75. 72. 74. 74. GooF 0.815 0.911 0.974 1.314 1.102 0.910 0.995 0.777 1.492 1.124 K 0.973 0.999 1.019 1.048 1.048 1.011 1.019 1.024 1.015 1.001 R1 0.085 0.072 0.070 0.082 0.053 0.045 0.051 0.021 0.039 0.020 Recommended weighting scheme: WGHT 0.0495 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -4 2 2 345.14 561.47 8.32 0.408 1.76 -1 5 7 10.91 19.19 4.22 0.075 1.01 1 1 0 115.07 140.48 3.98 0.204 5.28 2 6 3 165.08 26.17 3.68 0.088 1.04 -6 4 2 19.34 28.66 3.58 0.092 1.08 5 4 3 662.52 560.39 3.06 0.408 1.05 1 2 1 285.68 326.65 2.72 0.311 2.97 -2 1 6 246.38 215.83 2.71 0.253 1.61 6 4 2 32.47 39.23 2.71 0.108 1.00 -7 3 5 7.21 14.10 2.68 0.065 1.00 -2 0 10 39.64 23.40 2.60 0.083 1.01 -6 3 4 59.79 98.44 2.50 0.171 1.14 -4 3 8 19.33 25.74 2.32 0.087 1.05 1 4 1 51.93 44.66 2.29 0.115 1.68 1 4 7 55.95 15.64 2.25 0.068 1.06 6 2 0 254.32 225.97 2.24 0.259 1.24 -4 2 10 27.31 34.23 2.21 0.101 0.94 -6 2 9 34.47 41.90 2.21 0.112 0.93 2 1 7 60.82 75.03 2.19 0.149 1.21 0 3 8 14.57 19.46 2.18 0.076 1.08 -4 3 9 9.01 13.31 2.17 0.063 0.97 -1 6 7 -1.50 6.04 2.17 0.042 0.91 -4 5 6 12.45 17.07 2.16 0.071 1.01 -2 1 1 556.69 622.95 2.14 0.430 3.51 3 3 3 32.34 37.11 2.12 0.105 1.45 -8 2 6 72.47 82.95 2.12 0.157 0.93 -7 2 2 12.26 16.93 2.11 0.071 1.11 4 3 6 7.60 1.62 2.07 0.022 1.02 6 1 2 105.64 120.87 2.05 0.189 1.19 -6 2 5 59.84 126.25 2.05 0.194 1.18 3 1 2 179.88 162.75 2.01 0.220 2.03 -3 1 1 198.54 179.95 1.98 0.231 2.55 -1 0 6 23.80 30.32 1.97 0.095 1.68 1 2 0 292.23 321.30 1.92 0.309 3.22 -8 1 3 42.30 49.00 1.91 0.121 1.01 -4 0 8 27.90 33.76 1.91 0.100 1.18 -2 3 5 244.11 221.86 1.90 0.257 1.50 2 1 4 164.57 143.49 1.90 0.206 1.82 3 3 1 129.84 117.55 1.88 0.187 1.68 -3 2 8 254.19 230.19 1.87 0.261 1.16 2 6 2 29.00 33.51 1.86 0.100 1.08 1 6 2 113.15 133.80 1.86 0.199 1.12 3 3 7 82.65 97.47 1.86 0.170 1.01 -6 2 1 86.92 78.32 1.83 0.153 1.27 -5 4 7 53.56 62.09 1.83 0.136 1.00 -3 4 6 355.33 320.68 1.83 0.309 1.17 -3 4 9 20.27 14.62 1.81 0.066 0.94 -7 4 1 78.64 92.01 1.81 0.165 0.97 -7 3 2 16.87 11.64 1.80 0.059 1.05 -3 0 3 502.58 549.83 1.78 0.404 2.36 Bond lengths and angles C1 - Distance Angles O1B 1.2315 (0.0047) O1A 1.2696 (0.0045) 125.91 (0.34) C2 1.5527 (0.0052) 118.13 (0.30) 115.94 (0.28) C1 - O1B O1A C2 - Distance Angles O2A 1.2381 (0.0044) O2B 1.2702 (0.0047) 126.71 (0.37) C1 1.5527 (0.0052) 118.01 (0.32) 115.26 (0.30) C2 - O2A O2B O1A - Distance Angles C1 1.2696 (0.0045) O1A - O1B - Distance Angles C1 1.2315 (0.0047) O1B - O2A - Distance Angles C2 1.2381 (0.0044) O2A - O2B - Distance Angles C2 1.2702 (0.0047) O2B - C22 - Distance Angles N21 1.4886 (0.0050) C23 1.5094 (0.0055) 110.15 (0.31) H22A 0.9900 109.63 109.63 H22B 0.9900 109.63 109.63 108.15 C22 - N21 C23 H22A C23 - Distance Angles N24 1.4851 (0.0048) C22 1.5094 (0.0055) 110.03 (0.31) H23A 0.9900 109.65 109.65 H23B 0.9900 109.65 109.65 108.16 C23 - N24 C22 H23A C25 - Distance Angles N24 1.4847 (0.0049) C26 1.4953 (0.0052) 111.02 (0.30) H25A 0.9900 109.43 109.43 H25B 0.9900 109.43 109.43 108.03 C25 - N24 C26 H25A C26 - Distance Angles C25 1.4953 (0.0052) N21 1.5003 (0.0044) 110.19 (0.28) H26A 0.9900 109.62 109.62 H26B 0.9900 109.62 109.62 108.14 C26 - C25 N21 H26A C27 - Distance Angles N21 1.4951 (0.0047) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - N21 H27A H27B N21 - Distance Angles C22 1.4886 (0.0050) C27 1.4951 (0.0047) 112.63 (0.28) C26 1.5003 (0.0044) 109.63 (0.26) 111.53 (0.29) H21 0.9300 107.61 107.61 107.61 N21 - C22 C27 C26 N24 - Distance Angles C25 1.4847 (0.0049) C23 1.4851 (0.0048) 111.62 (0.28) H24A 0.9200 109.30 109.30 H24B 0.9200 109.30 109.30 107.96 N24 - C25 C23 H24A O1W - Distance Angles H1W 0.8474 (0.0206) H2W 0.8503 (0.0211) 104.76 (3.13) O1W - H1W O2W - Distance Angles H21W 0.8403 (0.0201) H22W 0.8647 (0.0205) 105.44 (2.94) O2W - H21W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.92 1.91 2.733(4) 147.1 N24-H24A...O1A 0.92 2.24 2.939(4) 132.0 N24-H24A...O2A 0.85(2) 1.88(3) 2.692(4) 159(6) O1W-H2W...O2B 0.84(2) 2.00(2) 2.787(4) 157(4) O2W-H21W...O2A 0.93 1.98 2.786(4) 143.8 N21-H21...O2B_$1 0.93 2.10 2.819(4) 133.3 N21-H21...O1B_$1 0.92 1.76 2.679(4) 178.3 N24-H24B...O1A_$2 0.85(2) 2.11(2) 2.934(4) 165(5) O1W-H1W...O2B_$3 0.86(2) 1.99(3) 2.797(4) 156(5) O2W-H22W...O1W_$3 FMAP and GRID set by program FMAP 2 2 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0462 for 738 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.16 at 0.2239 0.1187 0.6367 [ 1.51 A from H1W ] Deepest hole -0.17 at 0.5495 0.0790 0.5710 [ 0.80 A from H22A ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2280 / 13898 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2239 -0.3813 0.3633 1.00000 0.05 0.16 1.51 H1W 1.59 C2 1.69 O2A 1.85 O1W Q2 1 0.8041 0.1077 0.9666 1.00000 0.05 0.14 0.35 H25A 0.81 C25 1.53 H25B 1.70 N24 Q3 1 0.7311 0.5925 0.7020 1.00000 0.05 0.13 0.95 H27C 1.15 H27A 1.20 C27 2.06 H27B Q4 1 0.9249 0.3269 0.8243 1.00000 0.05 0.13 1.06 H21 1.28 O1B 1.58 N21 1.77 H26A Q5 1 0.1129 0.1786 0.9812 1.00000 0.05 0.13 1.18 O1B 1.38 C1 2.05 O1A 2.06 H26A Q6 1 -0.2854 -0.2065 0.4083 1.00000 0.05 0.12 1.21 O1W 1.53 H22W 1.60 H1W 1.95 H22B Q7 1 0.3734 -0.6666 0.7222 1.00000 0.05 0.12 1.47 H22W 1.82 O2W 1.83 H22B 1.97 H26B Q8 1 0.1637 -0.3510 0.6103 1.00000 0.05 0.12 1.20 H21W 1.45 H22W 1.62 O2W 2.40 H1W Q9 1 0.5027 0.3050 0.4865 1.00000 0.05 0.12 1.84 H22B 1.99 H22A 2.04 H23A 2.10 H27A Q10 1 0.4696 0.3131 0.9105 1.00000 0.05 0.12 1.34 O1A 1.43 H26B 1.86 H24A 1.90 H24B Shortest distances between peaks (including symmetry equivalents) 6 7 1.36 1 6 1.45 7 10 1.87 1 7 2.01 4 5 2.18 6 9 2.29 2 4 2.48 2 5 2.55 3 4 2.57 6 8 2.72 3 9 2.78 7 9 2.84 7 8 2.87 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.33: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.02: Generate idealized H-atoms 0.11: Structure factors and derivatives 0.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0059p21 finished at 08:44:05 Total CPU time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++